CN108190831B - A method of doping regulation hot melt Ag nanoparticle micro-nano interconnection line performance - Google Patents
A method of doping regulation hot melt Ag nanoparticle micro-nano interconnection line performance Download PDFInfo
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- 230000033228 biological regulation Effects 0.000 title claims abstract description 17
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- 239000002105 nanoparticle Substances 0.000 title description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 45
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- 239000002082 metal nanoparticle Substances 0.000 claims abstract description 13
- HKOOXMFOFWEVGF-UHFFFAOYSA-N phenylhydrazine Chemical compound NNC1=CC=CC=C1 HKOOXMFOFWEVGF-UHFFFAOYSA-N 0.000 claims abstract description 11
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- 238000005245 sintering Methods 0.000 claims abstract description 8
- -1 Dichlorodiphenyl Acetate silver Chemical compound 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims abstract description 4
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- 238000001914 filtration Methods 0.000 claims abstract description 3
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- 238000012545 processing Methods 0.000 claims description 4
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- 239000010949 copper Substances 0.000 description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 12
- 239000011701 zinc Substances 0.000 description 9
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- 238000005530 etching Methods 0.000 description 8
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- NIQQIJXGUZVEBB-UHFFFAOYSA-N methanol;propan-2-one Chemical compound OC.CC(C)=O NIQQIJXGUZVEBB-UHFFFAOYSA-N 0.000 description 6
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
- B82B3/0009—Forming specific nanostructures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
- B82B3/0061—Methods for manipulating nanostructures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
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Abstract
A kind of method of low-temperature-doped regulation hot melt Ag metal nanoparticle micro-nano interconnection line performance: (1) with lauryl amine and phenylhydrazine, Dichlorodiphenyl Acetate silver is restored in toluene, nano-Ag particles are obtained by filtration by G4 sand core funnel, obtain nano-Ag particles solution with organic solvent filter cartridge flushing；(2) dopant, ultrasonic disperse 2h will be added in the nano-Ag particles solution in step (1), the additional amount of dopant is the 1%~9% of silver amount；(3) by the liquid deposition of step (2) in the substrate etched, after the solvent of solution volatilizees completely naturally, the Argent grain other than substrate micro-structure is struck off, the nano grain of silver sub-line micro-structure adulterated；(4) by the product of step (3) in 100 ~ 180 DEG C of sintering 15min ~ 150min.The present invention improves the apparent form for interconnecting micro-structure and compactness and then the electric conductivity and mechanical performance that improve interconnection line to the regulation of the distribution size of grain growth size and micro- hole by being sintered.
Description
Technical field
The present invention relates to micron/nano manufacturing field more particularly to a kind of low-temperature-doped regulation hot melt Ag metal nanoparticles
The method of micro-nano interconnection line performance.
Background technique
Metal interconnecting wires are in semiconductor integrated circuit, solar battery, active matrix display device, Meta Materials micro-nano structure
Equal fields have a wide range of applications.
From aluminium interconnection technique to currently used copper interconnection technology, the development of related industry is pushed, but along with integrated
Circuit feature line width further decreases, and has been difficult to meet integrated circuit production using the Cu interconnection technique that Damascus technics is realized
The development of industry.Therefore, next-generation interconnection technique has been put on research schedule.
In next-generation interconnection material, Ag because of first choice as metal interconnecting wires the characteristics of its 52nm electron mean free path,
In the case where nanofeature line width strictly limits, it is possible to realize the ballistic transport of electronics in Ag metal interconnecting wires, improve
Interconnection line electric conductivity.In the technology of preparing of metal interconnection wire, based on metal micro-nano particle, metal is regulated and controled by doping
The hot melt of particle assistant metal particle linear is spread, in the side wall boundary of interconnection line, crystal boundary, micropore, surface topography
Etc. optimized, and then improve metal interconnecting wires electric conductivity and mechanical performance.The researchs such as Beijing Institute of Aeronautics great waves are in copper metal
In interconnection technology, Mg, Y metal fast decoupled facilitate Cu nanoparticle cluster fast nucleation and grow up, and Mg, Y play catalysis and make
With.There are also the reports that doping Mn regulates and controls Cu interconnection line metal grain size, doping P element regulation Cu interconnection line micropore size and distribution
Road.Tokyo University Komiyama. H et al. using Ti thin layer to the wellability of Cu, crystal orientation, partial size, interparticle distance, density etc. into
The apparent optimization of row.The researchs such as Sparz regulate and control the conductive characteristic of Cu film with Pt nanoparticle, regular hexagon short distance arrangement
Pt array of particles epitaxial growth Cu film, the temperature characterisitic for obtaining film resiativity meet F-S model, regularly arranged nanoparticle
Subarray reduces the random diffusing scattering of electronics.
Based on same physical mechanism, the Ag haveing excellent performance can equally be obtained by adulterating regulation based on Ag nanoparticle
Interconnection line.By the development of many years, copper interconnecting line technique has been the prevailing technology in modern integrated circuits interconnection field, and day
It is beneficial mature perfect, but copper wiring technique still remains many defects, with further decreasing and to mutual for characteristic size
Link current carrying density requirements greatly increase, and RC retardation ratio problem becomes increasingly conspicuous, and copper interconnecting line is also faced with conventional aluminum interconnection
Problem, interconnection line maximum current carrying density have been far from satisfying demand, and ELECTROMIGRATION PHENOMENON also more highlights.Under Ag is used as
Generation interconnection material, there is also some problems in metallic pseudoplastic fluid nano-imprint process: electric conductivity is poor,
Mechanical stability does not reach requirement, apparent form is coarse etc..
Summary of the invention
The purpose of the present invention is to provide a kind of low-temperature-dopeds to regulate and control hot melt Ag metal nanoparticle micro-nano interconnection line performance
Method.
Based on above-mentioned purpose, the present invention is adopted the following technical scheme that:
A kind of method of low-temperature-doped regulation hot melt Ag metal nanoparticle micro-nano interconnection line functional characteristic, including walk as follows
Rapid: (1) with lauryl amine and phenylhydrazine, Dichlorodiphenyl Acetate silver is restored in toluene, and nano-Ag particles are obtained by filtration by G4 sand core funnel, is used
Organic solvent filter cartridge flushing obtains nano-Ag particles solution；
(2) doping particle will be added in the nano-Ag particles solution in step (1), ultrasonic disperse 2h adulterates adding for particle
Enter 1%~9% that amount is silver amount；
(3) it by the liquid deposition of step (2) in the substrate etched, after the solvent of solution volatilizees completely naturally, strikes off
Argent grain other than substrate micro-structure, the nano grain of silver sub-line micro-structure adulterated；
(4) product of step (3) is sintered 15min ~ 150min at 100 ~ 180 DEG C up to the Nano silver grain micro-nano of doping
Interconnection line.
Further, detailed process is as follows for the reduction of Dichlorodiphenyl Acetate silver in toluene for lauryl amine and phenylhydrazine in the step (1):
Silver acetate, phenylhydrazine are dissolved in toluene respectively, the toluene solution of silver acetate is heated to 60 ± 5 DEG C, stirring is lower to be added
Enter lauryl amine, the toluene solution of phenylhydrazine is added dropwise after stirring evenly, the process temperature of dropwise addition is not less than 70 DEG C, is reacted after being added dropwise
Liquid, reacts 1 ~ 1.5 hour and temperature is reduced to 30 DEG C or less addition acetone and continues 5 ~ 15min of stirring, before the additional amount of acetone is
/ 5th of reaction solution volume are stated, addition volume ratio is 1:1 acetone methanol solution, is stirred 10 ~ 20 minutes, acetone methanol solution
Additional amount be previous reaction liquid product 5 times.
Preferably, the molar ratio of the silver acetate, phenylhydrazine and lauryl amine is 1 ︰, 0.5 ︰ (1.2 ~ 1.3).
Organic solvent in the step (1) is acetone.
Further, doping particle is selected from least one of following substances in the step (2):Zn、Mn、Ni、Fe、
Al,Cu,Y,Ti,Pt；The oxide of each metal of Zn, Mn, Ni, Fe, Al, Cu, Y, Ti, Pt.
Preferably, the additional amount of step (2) the doping particle is the 3%~7% of silver amount.
The substrate is silicon wafer, silica substrate or polytetrafluoroethylene (PTFE) substrate.
Sintering processing is hot plate conduction heating, baking oven heating, RTP heating or microwave heating.
It in the step (3), is performed etching using plasma etching machine, top electrode power 100kw, lower electrode power is
50kw, vacuum degree 5 × 10-3, etch period 800s, etching is three times.
In the above-mentioned methods, in the step (4), sintering processing should reach 180 DEG C using hot plate conduction heating temperature, when
Between be 2.5 hours；Oven heating temperature should be 160 DEG C, and the time should be 2 hours；RTP hot melting temperature is 140 DEG C, and the time is
0.5 hour；Microwave sintering temperature is 140 DEG C, and the time is 15 minutes.
In the above-mentioned methods, in the step (2), dopen Nano particle reduces the activation of nano silver due to its surface state
Can, high surface than, surface tension and capillary attraction after high surface energy, hot melt, increased based on mechanism Ag crystal grain such as hot melt diffusions,
Crystal boundary is reduced, micropore reduces and then keeps silver-colored interconnection line micro-structure surface smooth and then improve its electric conductivity, thermally conductive and mechanical performance.
The present invention is based on a certain proportion of regulation metal nano is added when preparing pseudoplastic behavior metal nanoparticle fluid
Particle or metal oxide component, the difference of diffusion velocity difference, activation energy and surface energy based on heterogeneous metal nanoparticle
Etc. factors, regulate and control the diffusion and fusion mechanism of metal nanoparticle；Optimize lines section micropore quantity and is uniformly distributed；Optimization is brilliant
Boundary's quantity and arrangement；Improve metal wire apparent roughness；Improve the consistency of metal connecting line unit volume；Inhibit doped alloys
The electromigration characteristic of micro-nano lines；Whole mechanical property, conductive characteristic and the heat-transfer character for promoting metal micro-nano interconnection line.
Compared with the existing technology the present invention has following gain effect:
The present invention improves interconnection micro-structure to the regulation of the distribution size of grain growth size and micro- hole by being sintered
Apparent form and compactness and then electric conductivity, mechanical performance and the thermal conduction characteristic for improving interconnection line, low-temperature rapid thermal is molten to be expanded
It dissipates and heat budget is greatly lowered.
Detailed description of the invention
Fig. 1 passes through the groove on the silicon wafer that dry plasma etch technique etches；
The Nano silver grain micro-nano interconnection line and fine silver of the doping Zn obtained of Fig. 2 embodiment 1 is sintered comparison diagram, and figure (a) is
The AFM figure of the Nano silver grain micro-nano interconnection line of Zn is adulterated, figure (b) is that the AFM of undoped nano silver micro-nano interconnection line schemes；From
Fig. 2 can be seen that keeps the surface topography of interconnection line micro-structure more preferable by adulterating regulation；
The change in resistance curve graph that the doping ratio of nickel made from Fig. 3 implementation 2 is 0%, 1%, 3%, 5%, 7%, 10%.
Specific embodiment
Below by specific embodiment, the present invention is further described, however, the present invention is not limited thereto.
Embodiment 1
A kind of method of low-temperature-doped regulation hot melt Ag metal nanoparticle micro-nano interconnection line performance, includes the following steps:
1, the presoma of nano silver micro-structure is prepared:
4.18g silver acetate is distributed to the toluene of 40mL, separately 1.35g phenylhydrazine is dissolved in 10mL toluene；
The toluene solution of silver acetate is heated to 60 DEG C, the lauryl amine of addition 6g under conditions of magnetic agitation, five minutes
The toluene solution of phenylhydrazine is added dropwise afterwards, the process temperature of time for adding 10min, dropwise addition are not less than 70 DEG C.React a hour and
The acetone that temperature is reduced to 30 DEG C of addition 10mL continues to stir 10min.Dose volume ratio is 1:1 acetone methanol mixed solution
The solution reacted is added acetone methanol solution, stirred 15 minutes by 100ml.It is filtered, is used in combination using the funnel of G4 model sand core
Acetone rinsing filter core obtains nano-Ag particles solution, is added the nanometer Zn particle that 0.134g will be adulterated, and ultrasonic disperse 2 hours；
2, nano silver interconnection line micro-structure is prepared: a layer photoresist in silicon wafer spin coating, with the exposure mask carving of certain line width
Draw the transition diagram of needs.It is performed etching using plasma etching machine, top electrode power 100kw, lower electrode power is
50kw, vacuum degree 5 × 10-3, etch period 800s, etching is three times；
3, nano silver is deposited: in the micro-structure after scattered Ag nano particles to be deposited on to silicon chip etching, nano silver
Grain in solution evaporation it is complete after remove the Argent grain other than micro-structure obtain adulterate Zn nano grain of silver sub-line micro-structure；
4, metal interconnecting wires are sintered: silicon wafer is put into accurate baking oven after being made and is sintered two for 160 DEG C by silver nanowires micro-structure
A hour is to obtain the Nano silver grain micro-nano interconnection line of doping Zn.
As shown in Fig. 2, the present embodiment is to adulterate particle to improve the apparent form of nano silver micro-structure with zinc, zinc is adulterated
Granular size of the size of sample particle obviously than undoped sample is bigger, and surface is more smooth.
Embodiment 2
A kind of method of low-temperature-doped regulation hot melt Ag metal nanoparticle micro-nano interconnection line performance, includes the following steps:
1, nano silver micro-structure presoma is prepared using chemical reduction method: 4.18g silver acetate is distributed to the toluene of 40mL,
Separately 1.35g phenylhydrazine is dissolved in 10mL toluene；
The toluene solution of silver acetate is heated to 60 DEG C, 6g lauryl amine is added under conditions of magnetic agitation, after five minutes
The toluene solution of phenylhydrazine is added dropwise, the process temperature of time for adding 10min, dropwise addition are not less than 70 DEG C.React a hour and temperature
The acetone that degree is reduced to 30 DEG C of addition 10mL continues to stir 10min.Dose volume ratio is 1:1 acetone methanol mixed solution 100ml,
Acetone methanol solution is added in the solution reacted, is stirred 15 minutes.It is filtered using the funnel of G4 model sand core, and is rushed with acetone
Filter wash core obtains nano-Ag particles solution；
Prepare 6 parts of above-mentioned nano-Ag particles solution, be added without metallic nickel respectively, silver amount is added 1%, 3%, 5%, 7%,
10% metallic nickel that will be adulterated, ultrasonic disperse 2 hours；
2, photoetching and etched mold: a layer photoresist in silicon wafer spin coating depicts needs with the mask plate of certain line width
Transition diagram.It is performed etching using plasma etching machine, top electrode power 100kw, lower electrode power 50kw, vacuum degree
5×10-3, etch period 800s, etching is three times；
3, nano silver is deposited: in the micro-structure after scattered Ag nano particles to be deposited on to silicon chip etching, nano silver
Grain in solution evaporation it is complete after remove the Argent grain other than micro-structure obtain adulterate Ni nano grain of silver sub-line micro-structure；
4, interconnection line is sintered: silver nanowires micro-structure puts in air atmosphere microwave agglomerating furnace silicon wafer into 140 DEG C after being made
Sintering 15 minutes to get to doping Ni Nano silver grain micro-nano interconnection line, wherein the doping ratio of nickel be 0%, 1%, 3%, 5%,
7%, 10%, the resistivity of each product is tested, concrete outcome is shown in Fig. 3.From the figure 3, it may be seen that the addition of metallic nickel improves silver-colored interconnection line
Conductive characteristic, nickel doping ratio be 5% when resistivity it is minimum.
Claims (4)
1. a kind of method of doping regulation hot melt Ag metal nanoparticle micro-nano interconnection line performance, which is characterized in that including as follows
Step:
(1) with lauryl amine and phenylhydrazine, Dichlorodiphenyl Acetate silver is restored in toluene, and nano-Ag particles are obtained by filtration by G4 sand core funnel, is used
Organic solvent filter cartridge flushing obtains nano-Ag particles solution；
(2) doping particle will be added in nano-Ag particles solution, ultrasonic disperse 2h, the additional amount for adulterating particle is the 1% of silver amount
~9%, the doping particle is Zn and/or Ni；
(3) by the liquid deposition of step (2) in the substrate etched, after the solvent of solution volatilizees completely naturally, substrate is struck off
Argent grain other than micro-structure, the nano grain of silver sub-line micro-structure adulterated；
(4) product of step (3) 15min ~ 150min is sintered at 100 ~ 180 DEG C to interconnect up to the Nano silver grain micro-nano of doping
Line.
2. the method for doping regulation hot melt Ag metal nanoparticle micro-nano interconnection line performance according to claim 1, special
Sign is that the additional amount of step (1) the doping particle is the 3%~7% of silver amount.
3. the method for doping regulation hot melt Ag metal nanoparticle micro-nano interconnection line performance according to claim 1, special
Sign is, when adulterating particle is Zn, sintering processing uses oven heating, and sintering temperature is 160 DEG C, and the time is 2 hours.
4. the method for doping regulation hot melt Ag metal nanoparticle micro-nano interconnection line performance according to claim 1, special
Sign is, when adulterating particle is Ni, sintering processing uses microwave heating, and sintering temperature is 140 DEG C, time 15min.
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| CN101622090A (en) * | 2007-02-27 | 2010-01-06 | 三菱麻铁里亚尔株式会社 | The synthetic method of dispersion solution of metal nanoparticle and preparation method thereof and metal nanoparticle |
| CN102500366A (en) * | 2011-11-03 | 2012-06-20 | 合肥美菱股份有限公司 | Photo-catalytic nanomaterial |
| CN103028728A (en) * | 2011-09-29 | 2013-04-10 | 三星电机株式会社 | Method of producing metal particles, and ink composition and paste composition produced by the same |
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| US5846288A (en) * | 1995-11-27 | 1998-12-08 | Chemet Corporation | Electrically conductive material and method for making |
| EP2444148A1 (en) * | 2010-10-25 | 2012-04-25 | Bayer Material Science AG | Metal particle sol with endowed silver nano particles |
| CN102809628B (en) * | 2012-05-29 | 2014-10-22 | 北京联合大学生物化学工程学院 | Nano-sensitive material for trimethylamine |
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|---|---|---|---|---|
| CN101622090A (en) * | 2007-02-27 | 2010-01-06 | 三菱麻铁里亚尔株式会社 | The synthetic method of dispersion solution of metal nanoparticle and preparation method thereof and metal nanoparticle |
| CN103028728A (en) * | 2011-09-29 | 2013-04-10 | 三星电机株式会社 | Method of producing metal particles, and ink composition and paste composition produced by the same |
| CN102500366A (en) * | 2011-11-03 | 2012-06-20 | 合肥美菱股份有限公司 | Photo-catalytic nanomaterial |
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